関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | p-Fluoronitrobenzene | HCID 9590 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | HCID 178418800 | HCID 178418800 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 4-Methyl-1-(4-nitrophenyl)-1H-imidazole | HCID 16005169 | 48.4% |
反応手順
4-fluoronitrobenzene (32.3 g; 0.229 mol) and 4-methyl-1H-imidazole (25 g; 0.3 mol) are mixed at r.t., to this stirred mixture K2CO3 (44 g; 0.3 mol) is added. The reaction mixture is then heated at 120° C. overnight, then cooled at r.t. and poured in water (2 L), the resulting suspension is filtered and washed with water. The obtained solid is dried at 60° C. and recrystallized from ethyl acetate (600 mL), to provide the title compound as a yellow solid (22.5 g; 48.3%). The regioisomer, 4-(5-methyl-1H-imidazol-1yl)nitrobenzene remains in the crystallization mother liquor along with a certain amount of the titled product (TLC: hexane/AcOEt 3:2). C10H9N3O2, MW 203.2.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08633208B2 |
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| 出典データセット | uspto-grants-2014_01 |
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| ORD ID | ord-467395d666b0426ab2aad45f8362ca2e |
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| 出典メモ | uspto-grants-2014_01 |
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